CN104488893A - Compound composition containing methanesulphonyl myclobutanil and plant growth regulator and preparation - Google Patents

Compound composition containing methanesulphonyl myclobutanil and plant growth regulator and preparation Download PDF

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CN104488893A
CN104488893A CN201410787905.8A CN201410787905A CN104488893A CN 104488893 A CN104488893 A CN 104488893A CN 201410787905 A CN201410787905 A CN 201410787905A CN 104488893 A CN104488893 A CN 104488893A
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plant growth
growth regulator
bacterium azoles
methylsulfonyl bacterium
preparation
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CN104488893B (en
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刘妤玲
何林师
李现玲
张青
杨家源
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Guangxi Tianyuan Biochemical Co Ltd
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Guangxi Tianyuan Biochemical Co Ltd
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Abstract

The invention provides a compound composition containing methanesulphonyl myclobutanil and a plant growth regulator and a preparation. The compound composition consists of the methanesulphonyl myclobutanil and the plant growth regulator, wherein the weight ratio of the methanesulphonyl myclobutanil to the plant growth regulator is (100:0.001)-(1:100); the chemical name of the methanesulphonyl myclobutanil is 2-(p-fluorophenyl)-5-methylsulfonyl-1,3,4-oxadiazole. The dosage form of a bactericide provided by the invention can be wettable powder, water dispersing granule, suspension, microemulsion, emulsion in water, granule or missible oil. The compound composition and the bactericide thereof have a remarkable synergetic effect in comparison with single dosage and are capable of effectively controlling various crop bacterial diseases and regulating the plants to grow healthily and strongly so as to achieve the benefits of improving the control efficiency, delaying the drug resistance, decreasing the medicament dosage, reducing the cost, improving the quality, keeping the output and increasing the output.

Description

A kind of complex composition and preparation containing methylsulfonyl bacterium azoles and plant growth regulator
Technical field
The present invention relates to technical field of pesticide, particularly relate to the complex composition of bactericide and plant growth regulator.
Background technology
Plant can be subject to causing harm of various disease and worm in process of growth, if prevent and treat not in time and supplement nutrient, growth regulation, often cause the underproduction in various degree, even No kernels or seeds are gathered, as in a year of scarcity, so while the sick worm of control is caused harm, also suitably should supplement nutrient, growth regulation, thus strengthen the resistivity of plant.In prior art, bactericide and plant growth regulator carry out now with the current, and the ratio that both use with does not have scientific basis, arbitrarily mix and not only do not reach synergistic effect, sometimes play antagonism on the contrary, waste medicament.
For this reason, Guizhou University's independent research also has the new type bactericide " one class preventing and control crop bacteriosis oxadiazole sulfone compound (patent No. is ZL201110314246.2) " of independent intellectual property rights, and its structural formula is:
The step of preparation process of this compound and condition:
(1) the different preparation replacing sour methyl ester intermediate: with different organic acids and absolute methanol for raw material, back flow reaction 6-10 hour under sulphuric acid catalysis, decompression separating methanol, after saturated sodium bicarbonate aqueous solution adjusts ph=7, separatory obtains different methyl formates;
(2) preparation of the different formylhydrazine intermediate replaced: be dissolved in methyl alcohol with different methyl formates, then slowly add 40%-80% hydrazine hydrate, till back flow reaction is complete, separates out the formylhydrazine of different replacement after cooling;
(3) 2-sulfydryl-5-replaces the preparation of-1,3,4-oxadiazole intermediate: with the formylhydrazine of above-mentioned preparation and KOH, carbon disulphide for raw material, ethanol is solvent, and back flow reaction is complete, de-ethanol, adjusts PH=5 to obtain 2-sulfydryl-5-and replaces-1,3,4-oxadiazole;
(4) 2-thioether-5-replaces-1,3, the preparation of 4-oxadiazole intermediate: replace-1 with above-mentioned 2-sulfydryl-5-, 3,4-oxadiazole is raw material, after the water-soluble solution of hydro-oxidation sodium, be obtained by reacting corresponding sulfide compound with 1-2 by the dimethyl sulfate of mole (second) ester or halogenated hydrocarbons etc.;
(5) 2-methyl (ethyl) sulfonyl-5-replaces the preparation of-1,3,4-oxadiazole.
With corresponding thioether for raw material, be dissolved in glacial acetic acid, 2%-7% potassium permanganate solution or 30% hydrogen peroxide oxidation obtain corresponding sulfone compound.
Plant growth regulator, it is a class agricultural chemicals of growing for coordinate plant growth, the compound comprising Prof. Du Yucang and the natural phytohormone extracted from biology, comprise brassin lactones, compound sodium nitrophenolate, diethyl aminoethyl hexanoate, the basic element of cell division, indolebutyric acid, Nafusaku, triacontanol, gibberellin, CPPU, paclobutrazol, heteroauxin, TrinexAN_SNacethyl, chlormequat, first piperazine, adjust naphthenic acid, oxyenadenine, Choline Chloride, inabenfide, 6-benzyl aminopurine etc.
Brassin lactones is known, English by name brassinolide, and it has physiological action widely, can obvious the growing of regulating plant.
Compound sodium nitrophenolate is known, English sodium nitrophenolate by name, its a kind of powerful cell-activating agent, with energy rapid permeability after plant contact in plant corpus, promotes the protoplasm flowing of cell, improves cell viability.Can rooting rate be accelerated, breaking dormancy, enhancing development, prevent fruit drop, improve product quality, improve output, improve disease-resistant, pest-resistant, the drought resisting of crop, waterlogging-resistant, cold-resistant, the anti-anti-adversity ability such as saline and alkaline, resistant to lodging.
Diethyl aminoethyl hexanoate (DA-6) has regulating action to plant growth, promotes plant cell division and growth, and tachyauxesis point breaks up; Promote seed germination, improve germination rate; Promote a point evil; Improve the activity of plant endoperoxide enzyme and nitrate reductase; The content of raising chlorophyll, protein, nucleic acid and photosynthetic rate; Improve the C N metabolism ratio in plant body, promote root system development; Also there is removing toxic substances more wound, short strong effect of recovery.
The basic element of cell division is the derivative of adenine (adenine), and mainly in tip of a root synthesis in plant corpus, upwards transport along xylem, phloem also can transport on a small quantity, can suppress the formation of side root and adventive root, promotes stomatal opening.
Indolebutyric acid is Endogenous auxin, can promote cell division and Growth of Cells, induced synthesis adventive root, increases setting, prevents shedding, changes female, male flower ratio etc.Can enter in plant corpus, with nutritional flow transporting to the position of working via blade, the tender epidermis of branch, seed.
Nafusaku is a broad spectrum type plant growth regulator, and it has action character and the physiological function of Endogenous auxin, can promote the formation of adventive root and root, accelerate cuttage root-taking and seed root of hair, division and the expansion of cell can be promoted, promote the differentiation of bud and bud, accelerate chlorophyllous synthesis, Fruit is impelled to prevent fruit drop, change the ratio of male and female flowering, and promote that plant root leaf is prosperous, improve output, oil recovery enhancement, strengthens drought resisting, the anti-adversity ability such as cold-resistant, disease-resistant.
Triacontanol is a kind of plant growth regulator of broad spectrum activity, can promote the growth of root system of plant, and have effect of increasing production.Triacontanol in the dark also can promote that protein synthesizes, and has that activity is low, physiological effect is strong, reaction velocity is fast, low-residual, non-harmful excellent characteristics, is naturally occurring, scope of application plant growth regulator quite widely.
Gibberellin is broad spectrum activity plant growth regulator, can promote cell, and stem extends, leaf expansion, and parthenocarpy, fruit growth, break seed dormancy, changes female, male flower ratio, affect flowering time, reduces flower, coming off really.Exogenous gibberellic acid enters in plant corpus, has the physiological function that endogenous gibberellins is same.
CPPU is a kind of efficient plant growth regulator, has cytokine activity.Can be passed through the root of plant, stem, leaf, bud, flower, fruit absorbs, and has enhancing photosynthesis, promotes that organelle is formed, breaks apical dominance, strengthen degeneration-resistant and anti-ageing different physiological roles of waiting for a long time.
Paclobutrazol is the inhibitor of endogenous hormones gibberellin synthesis, suppresses crop longitudinal tensile strain, makes to tiller or branch increases, and stem is thicker, and plant is downgraded compact, few mainly through Root Absorption, leaf absorptive amount, is not enough to cause metamorphosis, but can increases production.
Heteroauxin (IAA) synthesizes in the young leaflet tablet and apical meristem of expansion, and by the long-distance transportation of phloem, from top to down accumulates to base portion.Root also can produce growth hormone, transports from bottom to top.
TrinexAN_SNacethyl belongs to cyclohexane-carboxylic acid plant growth regulator, within 1992, goes on the market first by first just reaching in Switzerland, to cereal crop, castor-oil plant, paddy rice, the effect of sunflower display growth inhibition, can use and can prevent lodging after bud.
Chlormequat is a kind of excellent plant growth regulator, can be used for wheat; Paddy rice; Cotton; Tobacco; The crop such as corn and tomato, suppresses crop cell to extend, but not T suppression cell division, plant can be made to become short, bar stem is thicker, and leaf look turns green, and crop can be made drought-enduring waterlogging, prevents crop excessive growth from lodging, anti-saline and alkaline, the cotton shedding of cotton bolls can be prevented again, potato tubers can be made to increase.
First piperazine is new plant growth regulator, has good Uptake and translocation effect to plant.The reproductive growth of plant can be promoted; Suppress cauline leaf overgrowing, control side shoot, mould ideotype, improve root quantity and vigor, fruit is increased weight, quality improves.
Pyrrole acid is adjusted to be a kind of important plant growth regulator, for barley, paddy rice, wheat and turf, consumption 15 ~ 400g/ha.
Oxyenadenine belongs to cytokinin, is present in the fruit of plant seed, root, stem, leaf, young tender meristematic tissue and growth.Conduct to other positions primarily of tip of a root secretion, irritation cell divides, and promotes chlorophyll formation, prevents early ageing and fruit abscission, also can promote photosynthesis and protein synthesis, promote flower bud differentiation and formation.
Choline Chloride is a kind of plant photosynthesis promoter, has obvious effect to increase yield.
Inabenfide is a plant growth regulators, can suppress the synthesis of rice plant gibberellin, has the effect resistant to lodging of very strong selectivity to paddy rice.After application this product, every fringe Number of kernels reduces, but grain maturing rate improves, and actual production is increased.
6-benzyl aminopurine is the basic element of cell division of first man work synthesis, has the decomposition suppressing leaves of plants inner chlorophyll, nucleic acid, protein, protects green anti-old; Also to have amino acid, growth hormone, mineral salt etc. to multiple usefulness such as treatment sites allocation and transportation, be widely used in agricultural, fruit tree and horticultural crop each stage from germinateing to gathering in the crops.
Summary of the invention
Dui Yu oxadiazole sulfone compound, applicant researches and develops further, is selected from the fluorine in halogen atom, R as Rn 2select the methyl of C1-C5 alkyl and get the structural formula of oxadiazole sulfone compound:
Its chemical name is 2-(to fluorophenyl)-5-mesyl-1,3,4-oxadiazole, is called for short methylsulfonyl bacterium azoles.
The concrete syntheti c route of compound methylsulfonyl bacterium azoles is as follows:
(1) to the synthesis of fluorobenzoyl hydrazine
(2) 2-sulfydryl-5-is to the synthesis of fluorophenyl-1,3,4-oxadiazole
(3) 2-Dimethyl sulfide-5-is to the synthesis of fluorophenyl-1,3,4-oxadiazole
(4) 2-(to fluorophenyl)-5-mesyl-1,3,4-oxadiazole target compound is prepared
Applicant studies discovery further, and methylsulfonyl bacterium azoles is the control bacterial disease medicament of novel structure, by suppressing the synthesis of pathogene energy, the growth of anti-bacteria and breeding.Methylsulfonyl bacterium azoles has the feature of interior suction, conduction, and after infiltration blade epidermis, energy transporting is to other positions of same blade.A large amount of isolated tests shows, methylsulfonyl bacterium azoles has good inhibitory action to causing the various pathogenetic bacterias of phytobacterial disease, and namely directly anti-bacteria is bred.Through repeatedly pot experiment and field control effectiveness test checking, show that methylsulfonyl bacterium azoles all has good control efficiency to crop bacterial disease, especially good control effect is all had to bacterial blight of rice, slice disease, tobacco bacterial wilt, bacterial wilt of tomato, citrus bacterial canker disease etc., and plant growth can be stimulated to a certain extent healthy and strong, improve the resistance of crop.This compound has efficiently, the feature of wide spectrum, use safety, is a bactericide having much exploitation potential quality.Find through test, methylsulfonyl bacterium azoles and plant growth regulator mixture control corps diseases effect very outstanding.
In view of this, for the deficiency that prior art exists, the object of the invention is to provide a kind of complex composition and the preparation thereof that contain methylsulfonyl bacterium azoles and plant growth regulator, this complex composition and preparation thereof have obvious synergistic effect relative to single dose, improve bactericidal effect, promote that plant growth is healthy and strong, strengthen the anti-adversity ability of crop, improve crop quality, protect and produce volume increase.
To achieve these goals, the technical solution used in the present invention is:
The invention provides a kind of complex composition containing methylsulfonyl bacterium azoles and plant growth regulator, described complex composition is made up of methylsulfonyl bacterium azoles and plant growth regulator, the chemical name of described methylsulfonyl bacterium azoles is 2-(to fluorophenyl)-5-mesyl-1, 3, 4-oxadiazole, described plant growth regulator is brassin lactones, compound sodium nitrophenolate, diethyl aminoethyl hexanoate, the basic element of cell division, indolebutyric acid, Nafusaku, triacontanol, gibberellin, CPPU, paclobutrazol, heteroauxin, TrinexAN_SNacethyl, chlormequat, first piperazine, adjust naphthenic acid, oxyenadenine, Choline Chloride, inabenfide, any one in 6-benzyl aminopurine.
The above-described complex composition containing methylsulfonyl bacterium azoles and plant growth regulator, in order to ensure to have good control efficiency and synergistic effect, as preferably, described methylsulfonyl bacterium azoles and the weight ratio of plant growth regulator are 100:0.001 to 1:100.
Any described complex composition containing methylsulfonyl bacterium azoles and plant growth regulator above, in order to ensure to have good control efficiency and synergistic effect, as preferably, described methylsulfonyl bacterium azoles and the weight ratio of plant growth regulator are 100:0.01 to 1:30.
Contain a preparation for methylsulfonyl bacterium azoles and plant growth regulator, described preparation comprises acceptable auxiliary material on above arbitrary described complex composition and agricultural chemicals, is then prepared into disinfectant use in agriculture.
The above-described preparation containing methylsulfonyl bacterium azoles and plant growth regulator, by weight, the weight percentage that described complex composition accounts for described bactericide is 0.1%-80%.
The above-described preparation containing methylsulfonyl bacterium azoles and plant growth regulator, by weight, the weight percentage that described complex composition accounts for described bactericide is 1%-65%.
The above-described preparation containing methylsulfonyl bacterium azoles and plant growth regulator, on described agricultural chemicals, acceptable auxiliary material is the mixture of a kind of and auxiliary agent in solvent and filler.
Arbitrary described preparation containing methylsulfonyl bacterium azoles and plant growth regulator above, the formulation of described bactericide is wetting powder, water dispersible granules, microemulsion, aqueous emulsion, missible oil, suspending agent or granule.
In embodiments more provided by the invention, described auxiliary agent comprises surfactant, wetting dispersing agent, also can add other conventional functionality auxiliary agents such as antifreezing agent, thickener, stabilizing agent, defoamer, disintegrant, film forming agent if desired.
In embodiments more provided by the invention, surfactant used comprises non-ionic surface active agent, anion surfactant.
Non-ionic surface active agent is ethylene oxide adduct, high-carbon fatty alcohol polyoxyethylene ether, fatty acid methyl ester ethoxylate, alkylphenol polyoxyethylene, the polyoxyethylene sorbitan fatty acid ester of polypropylene glycol, fatty alcohol-polyoxyethylene ether, condensation compound of alkyl phenol and epoxy ethane, polyoxyethylene nonylphenol ether, triphen ethyl phenol APEO, two phenethyl phenol polyethenoxy ether.
Anion surfactant is calcium dodecyl benzene sulfonate, branch-alkylbenzene sulfonate, sodium alkyl benzene sulfonate, fatty alcohol sulfate monoethanolamine salt.
Wetting dispersing agent is alkyl benzene sulfonate calcium salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, polyoxyethylene carboxylate, condensation compound of methyl naphthalene sulfonic acid and formaldehyde sulphate, naphthalene sulfonic acid-formaldehyde condensation product, methanonaphthalene sodium sulfonate, dibutyl naphthalenesulfonic acid formaldehyde condensation products, N-Methyl fatty acyl taurines sodium, alkylphenol polyoxyethylene formaldehyde condensation products sulphate, alkylphenol polyoxyethylene phosphate, the withered powder of tea, saponin, lignosulfite, aliphatic alcohol sulfate, dodecyl sodium sulfate, fatty acid amide-N methyl taurine sodium salt, sodium sulfate of polyethenoxy ether of fatty alcohol, pull open powder.
Solvent is one or more in methyl alcohol, ethanol, solvent naphtha, castor oil, soybean oil, turpentine oil, eucalyptus oil, trimethylbenzene, dimethylbenzene, dimethyl formamide, dromisol, N methyl pyrrolidone, glycol dimethyl ether and methyl oleate.
Solid packing is one or more in imvite, clay, earth powder, diatomite, atlapulgite, kaolin, attapulgite, gypsum, potter's clay, talcum powder and precipitated calcium carbonate.
Antifreezing agent is ethylene glycol, isopropyl alcohol, n-butanol, propane diols, glycerine, one or more in urea.
Disintegrant is sodium sulphate, ammonium chloride, sodium phosphate, ammonium sulfate, urea, potash, sodium chloride, potassium sulfate, potassium nitrate, potassium phosphate.
Thickener is polyvinylpyrrolidone, xanthans, aluminium-magnesium silicate, polyvinyl alcohol and polyvinyl acetate.
According to different requirements, the formulation of bactericide of the present invention is the preparation of wetting powder, suspending agent, microemulsion, missible oil, aqueous emulsion, water dispersible granules, granule, seed coat agent, soluble powder, soluble liquid, suspension emulsion, dry suspending agent, ultra low volume liquids or other formulation.
In embodiments more provided by the invention, the formulation of bactericide of the present invention is preferably wetting powder, water dispersible granules, microemulsion, aqueous emulsion, missible oil, suspending agent or granule.
Complex composition of the present invention can be used by commonsense method, as spraying cauline leaf process, also can soil treatment, and such as solid root spreads fertilizer over the fields or liquid fills with root, can also dress seed, to soak seed or seed pelleting uses.
Above-mentioned complex composition can be used for control crop bacterial disease.
Described bacterial disease can be spotted type bacteriosis, leaf withered type bacteriosis, blue or green withered type bacteriosis, withered type bacteriosis, ulcer type bacteriosis, type bacteriosis of rotting or deformity bacteriosis.
Above-mentioned spotted type bacteriosis is paddy bacterial brown spot, bacterial leaf streak of rice, cucumber bacterial angular leaf spot, cotton bacterial angular leaf spot, tomato macula disease, Chinese cabbage leaf spot, watermelon bacterial angular leaf spot, cucumber bacterial angular leaf spot, pepper bacterial leaf spot, Chinese cabbage bacterial angular leaf spot, mango bacterial black spot, common bacterial blight of bean or corn bacterial leaf blight;
The withered type bacteriosis of above-mentioned leaf is bacterial blight of rice, cucumber Bacterial Leaf Blight, konjaku Bacterial Leaf Blight or cucumber leaf rot;
The withered type bacteriosis of above-mentioned green grass or young crops is tobacco bacterial wilt, bacterial wilt of tomato, potato bacterial wilt, leather certain kind of berries bacterial wilt, pepper ralstonia solanacearum or eggplant bacterial wilt;
Above-mentioned withered type bacteriosis is potato wilt;
Above-mentioned ulcer type bacteriosis is citrus ulcer, bacterial pustule of soybean, canker of tomato, tomato shot hole, bacterial speck or bacterial spot of pepper;
Above-mentioned rotten type bacteriosis is the bacterial slimy soft rot of Solanaceae and ground family crop, paddy rice basal stem rot, soft rot of cabbage, capsicum soft rot, wild cabbage soft rot, cabbage black rot, potato bacterial ring rot or bacterial soft rot of potato.
In embodiments more provided by the invention, described complex composition can be used for high-efficiency prevention and control cucumber bacterial angular leaf spot, citrus bacterial canker disease, paddy bacterial angular leaf spot, bacterial wilt of tomato.
Complex composition provided by the invention and bactericide have the following advantages relative to prior art tool:
Synergistic effect is obvious, and test shows that methylsulfonyl bacterium azoles and the composite bactericide of plant growth regulator have good synergistic effect in controlling disease, not only increases control efficiency, also reduces the usage amount of medicament.
Protect to greatest extent and produce volume increase: in process of crop growth, the harm of bacterial disease, must affect the growing way of crop, and if can while controlling disease, regulate the balance of plant physiology metabolism and nutrient in time, then can protect to greatest extent and produce volume increase.
Embodiment
Below by embodiment, the present invention is further elaborated.It should be noted that, the embodiment of the present invention is only used for the present invention is described, instead of limitation of the present invention.The former medicine of methylsulfonyl bacterium azoles used in the present invention is provided by Guizhou University, and other former medicines used and preparation are commercial.
Embodiment prepared by preparation:
One, the preparation of microemulsion
Preparation technology: add in solvent by methylsulfonyl bacterium azoles and plant growth regulator, obtains transparent mixed liquor after stirring; In above-mentioned mixed liquor, add surfactant, be stirred to surfactant and dissolve completely; Under the mixing speed of 50r/min, the water of surplus is joined and is above-mentionedly dissolved with in the mixed liquor of surfactant, at ambient temperature, stir 30min, obtain the microemulsion of homogeneous transparent; In above-mentioned microemulsion, add antifreezing agent, stir, obtain the microemulsion of bactericide of the present invention.
Formula composition:
Two, the preparation of wetting powder
Preparation technology: methylsulfonyl bacterium azoles, plant growth regulator, wetting dispersing agent, white carbon, filler are mixed, after airslide disintegrating mill is pulverized, stirs 30min, obtains the wetting powder of bactericide of the present invention.
Three, the preparation of suspending agent
Preparation technology: by antifreezing agent, thickener, surfactant, moisture content mixing, mix through high speed shear, add methylsulfonyl bacterium azoles, plant growth regulator successively, abrading-ball 2 ~ 3 hours in ball crusher, the suspending agent of obtained bactericide of the present invention
Four, the preparation of aqueous emulsion
Preparation technology: by methylsulfonyl bacterium azoles and plant growth regulator, surfactant, solvent, be dissolved into uniform oil phase; Part water, antifreezing agent are mixed uniformly aqueous phase; While high-speed stirred, oil phase is added aqueous phase in a kettle., opens clipper and carry out high speed shear, and add remaining water and supply, shear about half an hour, namely obtained bactericide of the present invention aqueous emulsion.
Five, the preparation of water dispersible granules
Preparation technology: methylsulfonyl bacterium azoles, plant growth regulator, wetting dispersing agent, white carbon, filler are mixed, after airslide disintegrating mill is pulverized, stir 30min, through mediating, after add in fluidized-bed granulation dryer and carry out granulation, drying, obtain the water dispersible granules of bactericide of the present invention.
Six, the preparation of missible oil
Preparation technology: add in solvent by methylsulfonyl bacterium azoles and plant growth regulator, obtains transparent mixed liquor after stirring, i.e. the missible oil of obtained bactericide of the present invention
Seven, granule
By each for following table component Homogeneous phase mixing, air-flow crushing, adds suitable quantity of water and mediates, and the mixture pelleting of gained, is drying to obtain the granule of bactericide of the present invention.
The present composition, except can being made into above formulation, can also make the multiple formulations such as seed coat agent, micro-capsule suspension, injection drying agent, ultra low volume.
BIOLOGICAL ACTIVITY EXAMPLES
In order to clear and definite methylsulfonyl bacterium azoles and plant growth regulator alone with time mixed to the control efficiency of several bacterial disease and fungal disease, We conducted Toxicity Determination and field control effectiveness test.
Toxicity Determination:
Following indoor biometrics test adopts the abundant method of Sun Yun to calculate co-toxicity coefficient (CTC) and evaluates mixed effect.
Toxicity index TI (B)=(EC of standard agent A 50the EC of ÷ B agent 50) × 100
Actual toxicity index ATI (AB)=(EC of A 50the EC of ÷ AB 50) × 100
Theoretical toxicity index TTI (AB)=TI (the A) × A percentage+TI (B) in the mixture × percentage of B in mixture
Actual measurement toxicity index (ATI)=(standard agent EC 50÷ reagent agent EC 50) × 100
In theoretical toxicity index (TTI)=A medicament toxicity index × mixture A percentage composition+B medicament toxicity index × mixture in the percentage composition of B
Co-toxicity coefficient (CTC)=[the theoretical toxicity index (TTI) of mixture actual measurement toxicity index (ATI) ÷ mixture] × 100
Evaluation criterion is: co-toxicity coefficient >=120 show as synergistic effect; Co-toxicity coefficient≤80 show as antagonism; 80< co-toxicity coefficient <120 shows as summation action.
Toxicity Determination embodiment one: (bacterial leaf streak of rice)
Below that methylsulfonyl bacterium azoles is tested the Toxicity Determination of bacterial leaf streak of rice with brassin lactones, triacontanol, gibberellin, TrinexAN_SNacethyl, chlormequat respectively.
Adopt in vitro nephelometry to carry out Toxicity Determination, select bacterial leaf streak of rice to be target target, repeat 4 times, latter 24 hours check results of investigating.Be independent variable x with drug concentration (mg/l) logarithm value, with the probit value of the corrected mortality of its correspondence for dependent variable y, set up virulence regression equation respectively, obtain the co-toxicity coefficient of two single dose different ratio.Experimental technique adopts the abundant method of Sun Yun to calculate co-toxicity coefficient (CTC) and evaluates mixed effect.
Concrete grammar: adopt in vitro Nephelometric Determination, design concentration on the basis of preliminary experiment, each medicament is joined respectively in NA liquid nutrient medium, gradient dilution makes pastille medium, Inoculated Rice Xanthomonas campestris PV.oryzicola is placed on 28 DEG C of about shaken cultivation 24h, its turbidity (turbidity and bacterium amount be changing into positive correlation) is measured with transmissometer, the inhibiting rate that each chemicals treatment breeds bacterial growth is calculated according to the turbidity of blank and the turbidity of process, by the linear regression analysis between the probit value of inhibiting rate and the logarithm value of serial drug concentration, obtain the EC of each medicament 50value, CTC value.The results are shown in Table 1 ~ table 5.
The Toxicity Determination result of table 1 methylsulfonyl bacterium azoles and the composite control bacterial leaf streak of rice of brassin lactones
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 7.16 100.00 / /
Brassin lactones (hereinafter referred to as B) 74.39 9.62 / /
A:B=100000:1 5.94 120.54 100.00 120.54
A:B=60000:1 5.21 137.43 100.00 137.43
A:B=30000:1 5.02 142.63 100.00 142.63
A:B=10000:1 4.47 160.18 99.99 160.19
A:B=6000:1 4.31 166.13 99.98 166.15
A:B=3000:1 4.28 167.29 99.97 167.34
A:B=1000:1 4.12 173.79 99.91 173.94
A:B=600:1 4.06 176.35 99.85 176.62
A:B=300:1 3.84 186.46 99.70 187.02
A:B=100:1 3.62 197.79 99.11 199.58
A:B=60:1 3.58 200.00 98.52 203.01
A:B=30:1 3.69 194.04 97.08 199.86
A:B=15:1 4.06 176.35 94.35 186.91
A:B=5:1 4.69 152.67 84.94 179.74
A:B=1:1 7.39 96.89 54.81 176.76
A:B=1:5 16.89 42.39 24.69 171.71
A:B=1:15 28.26 25.34 15.27 165.88
A:B=1:30 35.27 20.30 12.54 161.88
A:B=1:60 49.35 14.51 11.11 130.63
A:B=1:100 53.26 13.44 10.52 127.79
The Toxicity Determination result of table 2 methylsulfonyl bacterium azoles and the composite control bacterial leaf streak of rice of triacontanol
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 6.32 100.00 / /
Triacontanol (hereinafter referred to as I) 84.77 7.46 / /
A:I=100000:1 5.23 120.84 100.00 120.84
A:I=60000:1 4.33 145.96 100.00 145.96
A:I=30000:1 4.21 150.12 100.00 150.12
A:I=10000:1 3.86 163.73 99.99 163.75
A:I=6000:1 3.80 166.32 99.98 166.34
A:I=3000:1 3.56 177.53 99.97 177.58
A:I=1000:1 3.41 185.34 99.91 185.51
A:I=600:1 3.34 189.22 99.85 189.51
A:I=300:1 3.24 195.06 99.69 195.66
A:I=100:1 2.71 233.21 99.08 235.37
A:I=60:1 3.17 199.37 98.48 202.44
A:I=30:1 3.69 171.27 97.01 176.54
A:I=15:1 3.82 165.45 94.22 175.60
A:I=5:1 4.37 144.62 84.58 171.00
A:I=1:1 7.06 89.52 53.73 166.61
A:I=1:5 16.76 37.71 22.88 164.81
A:I=1:15 29.25 21.61 13.24 163.20
A:I=1:30 37.40 16.90 10.44 161.85
A:I=1:60 47.45 13.32 8.97 148.44
A:I=1:100 62.70 10.08 8.37 120.40
The Toxicity Determination result of table 3 methylsulfonyl bacterium azoles and the composite control bacterial leaf streak of rice of gibberellin
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 6.99 100.00 / /
Gibberellin (hereinafter referred to as J) 68.29 10.24 / /
A:J=100000:1 5.77 121.14 100.00 121.14
A:J=60000:1 5.04 138.69 100.00 138.69
A:J=30000:1 4.88 143.24 100.00 143.24
A:J=10000:1 4.31 162.18 99.99 162.20
A:J=6000:1 4.24 164.86 99.99 164.88
A:J=3000:1 4.18 167.22 99.97 167.27
A:J=1000:1 3.96 176.52 99.91 176.67
A:J=600:1 3.74 186.90 99.85 187.18
A:J=300:1 3.59 194.71 99.70 195.29
A:J=100:1 3.27 213.76 99.11 215.68
A:J=60:1 3.35 208.66 98.53 211.77
A:J=30:1 3.50 199.71 97.10 205.67
A:J=15:1 3.81 183.46 94.39 194.37
A:J=5:1 4.71 148.41 85.04 174.52
A:J=1:1 7.46 93.70 55.12 170.00
A:J=1:5 16.63 42.03 25.20 166.82
A:J=1:15 26.75 26.13 15.85 164.90
A:J=1:30 33.25 21.02 13.13 160.09
A:J=1:60 45.78 15.27 11.71 130.42
A:J=1:100 50.81 13.76 11.12 123.67
The Toxicity Determination result of table 4 methylsulfonyl bacterium azoles and the composite control bacterial leaf streak of rice of Lodging-proof agent
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 6.27 100.00 / /
TrinexAN_SNacethyl (hereinafter referred to as T) 72.36 8.67 / /
A:T=100000:1 4.96 126.41 100.00 126.41
A:T=60000:1 4.50 139.33 100.00 139.34
A:T=30000:1 4.46 140.58 100.00 140.59
A:T=10000:1 3.86 162.44 99.99 162.45
A:T=6000:1 3.69 169.92 99.98 169.94
A:T=3000:1 3.59 174.65 99.97 174.70
A:T=1000:1 3.24 193.52 99.91 193.70
A:T=600:1 3.13 200.32 99.85 200.62
A:T=300:1 2.80 223.93 99.70 224.61
A:T=100:1 3.00 209.00 99.10 210.91
A:T=60:1 3.46 181.21 98.50 183.97
A:T=30:1 3.55 176.62 97.05 181.98
A:T=15:1 3.70 169.46 94.29 179.72
A:T=5:1 4.31 145.48 84.78 171.60
A:T=1:1 6.82 91.94 54.33 169.21
A:T=1:5 16.03 39.11 23.89 163.74
A:T=1:15 26.81 23.39 14.37 162.71
A:T=1:30 33.75 18.58 11.61 160.00
A:T=1:60 45.74 13.71 10.16 134.89
A:T=1:100 52.92 11.85 9.57 123.81
The Toxicity Determination result of table 5 methylsulfonyl bacterium azoles and the composite control bacterial leaf streak of rice of chlormequat
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 6.58 100.00 / /
Chlormequat (hereinafter referred to as O) 79.37 8.29 / /
A:O=100000:1 5.41 121.63 100.00 121.63
A:O=60000:1 4.71 139.70 100.00 139.70
A:O=30000:1 4.50 146.22 100.00 146.23
A:O=10000:1 4.09 160.88 99.99 160.89
A:O=6000:1 3.70 177.84 99.98 177.87
A:O=3000:1 3.55 185.35 99.97 185.41
A:O=1000:1 3.49 188.54 99.91 188.71
A:O=600:1 3.31 198.79 99.85 199.10
A:O=300:1 3.12 210.90 99.70 211.54
A:O=100:1 3.29 200.00 99.09 201.83
A:O=60:1 3.42 192.40 98.50 195.33
A:O=30:1 3.75 175.47 97.04 180.82
A:O=15:1 3.94 167.01 94.27 177.16
A:O=5:1 4.57 143.98 84.72 169.96
A:O=1:1 7.23 91.01 54.15 168.08
A:O=1:5 17.11 38.46 23.58 163.12
A:O=1:15 28.87 22.79 14.02 162.54
A:O=1:30 36.16 18.20 11.25 161.77
A:O=1:60 46.17 14.25 9.79 145.52
A:O=1:100 58.99 11.15 9.20 121.27
1-5 is visible for toxicity test result table, methylsulfonyl bacterium azoles respectively with brassin lactones, triacontanol, gibberellin, TrinexAN_SNacethyl, chlormequat in (100000 ~ 1): (1: ~ 100) in scope, the co-toxicity coefficient of composite control bacterial leaf streak of rice is all greater than 120, shows obvious synergistic function.Especially in (10000 ~ 1): time composite in (1 ~ 30) scope, the CTC of each process is all greater than 160, and synergy is particularly remarkable.
Toxicity Determination embodiment two: (soft rot of cabbage)
Be below methylsulfonyl bacterium azoles respectively with paclobutrazol, heteroauxin, first piperazine, adjust the composite Toxicity Determination to soft rot of cabbage of naphthenic acid to test.
Bacterium solution preparation: bacterial classification cultured in test tube is extracted test tube tampon near alcolhol burner place, pour 10ml sterile water into, with disinfection inoculation pin, germ on inclined-plane is scraped gently, make spore suspension, being poured into by this spore suspension is equipped with in the sterilizing triangular flask of several glass marbles in advance again, cross bacteriological filtration liquid with sterile gauze after shake 5min, put in another sterilizing triangular flask, namely make required bacterium liquid.
Concrete grammar: by beef extract-peptone agar medium melt, to be cooled to 45 DEG C ~ 50 DEG C time, aseptically pour into rapidly in sterilizing culture dish together with 0.2ml bacterial suspension, every ware 15ml medium, shakes up rear cooled and solidified.With card punch (aperture 4mm) punching after sterilizing, 1ml liquid is dripped in circular hole, be placed in after 28 DEG C of insulating boxs cultivate 2d, measure 2 diameters of inhibition zone by right-angled intersection method with slide measure, average, calculate inhibiting rate, obtain virulence curve and EC 50, and press Sun Yun abundant method calculating co-toxicity coefficient.The results are shown in Table 6 ~ table 9.
Table 6 methylsulfonyl bacterium azoles and the composite Toxicity Determination result of preventing and treating soft rot of cabbage of paclobutrazol
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 7.42 100.00 / /
Paclobutrazol (hereinafter referred to as L) 76.23 9.73 / /
A:L=100000:1 6.02 123.26 100.00 123.26
A:L=55000:1 5.54 133.94 100.00 133.94
A:L=25000:1 5.01 148.10 100.00 148.11
A:L=10000:1 4.58 162.01 99.99 162.02
A:L=5500:1 4.37 169.79 99.98 169.82
A:L=2000:1 4.32 171.76 99.95 171.84
A:L=900:1 4.20 176.67 99.90 176.84
A:L=550:1 4.19 177.09 99.84 177.38
A:L=200:1 3.84 193.23 99.55 194.10
A:L=90:1 3.78 196.30 99.01 198.26
A:L=50:1 4.11 180.54 98.23 183.79
A:L=25:1 4.25 174.59 96.53 180.87
A:L=12:1 4.44 167.12 93.06 179.59
A:L=4:1 5.16 143.80 81.95 175.48
A:L=1:1 8.05 92.17 54.87 168.00
A:L=1:4 16.20 45.80 27.79 164.83
A:L=1:15 29.69 24.99 15.38 162.54
A:L=1:30 36.50 20.33 12.65 160.76
A:L=1:60 46.42 15.98 11.21 142.55
A:L=1:100 57.98 12.80 10.63 120.42
Table 7 methylsulfonyl bacterium azoles and the composite Toxicity Determination result to soft rot of cabbage of heteroauxin
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 6.83 100.00 / /
Heteroauxin (hereinafter referred to as M) 79.45 8.60 / /
A:M=100000:1 5.40 126.48 100.00 126.48
A:M=55000:1 4.91 139.10 100.00 139.11
A:M=25000:1 4.59 148.80 100.00 148.81
A:M=10000:1 4.24 161.08 99.99 161.10
A:M=5500:1 4.20 162.62 99.98 162.65
A:M=2000:1 3.89 175.58 99.95 175.66
A:M=900:1 3.64 187.64 99.90 187.83
A:M=550:1 3.44 198.55 99.83 198.88
A:M=200:1 3.03 225.41 99.55 226.44
A:M=90:1 3.24 210.80 99.00 212.94
A:M=50:1 3.61 189.20 98.21 192.65
A:M=25:1 3.74 182.62 96.48 189.27
A:M=12:1 3.91 174.68 92.97 187.89
A:M=4:1 4.90 139.39 81.72 170.57
A:M=1:1 7.52 90.82 54.30 167.27
A:M=1:4 15.31 44.61 26.88 165.98
A:M=1:15 29.22 23.37 14.31 163.35
A:M=1:30 36.72 18.60 11.55 161.11
A:M=1:60 45.95 14.86 10.10 147.24
A:M=1:100 57.06 11.97 9.50 125.98
Table 8 methylsulfonyl bacterium azoles and the composite Toxicity Determination result of preventing and treating soft rot of cabbage of first piperazine
Composition EC 50, (, μ g/ml, ), ATITTICTC methylsulfonyl bacterium azoles, (, hereinafter referred to as A, ), 6.39100.00//first piperazine, (, hereinafter referred to as P, ), 80.227.97//A:P=100000:15.15124.08100.00124.08A:P=55000:14.44143.92100.00143.92A:P=25000:14.26150.00100.00150.01A:P=10000:13.81167.7299.99167.73A:P=5500:13.72171.7799.98171.80A:P=2000:13.62176.5299.95176.60A:P=900:13.58178.4999.90178.67A:P=550:13.37189.6199.83189.93A:P=200:12.35271.9199.54273.17A:P=90:12.98214.4398.99216.62A:P=50:13.22198.4598.20202.09A:P=25:13.35190.7596.46197.75A:P=12:13.88164.6992.92177.24A:P=4:14.61138.6181.59169.88A:P=1:17.0390.9053.98168.38A:P=1:414.8143.1526.37163.60A:P=1:1528.5922.3513.72162.93A:P=1:3036.1317.6910.93161.75A:P=1:6045.9113.929.47146.91A:P=1:10056.1611.388.88128.18
Table 9 methylsulfonyl bacterium azoles and the composite Toxicity Determination result of preventing and treating soft rot of cabbage of tune naphthenic acid
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 7.16 100.00 / /
Adjust naphthenic acid (hereinafter referred to as Q) 75.33 9.50 / /
A:Q=100000:1 5.84 122.60 100.00 122.60
A:Q=55000:1 5.00 143.20 100.00 143.20
A:Q=25000:1 4.86 147.33 100.00 147.33
A:Q=10000:1 4.47 160.18 99.99 160.19
A:Q=5500:1 4.26 168.08 99.98 168.10
A:Q=2000:1 4.13 173.37 99.95 173.44
A:Q=900:1 3.95 181.27 99.90 181.45
A:Q=550:1 3.84 186.46 99.84 186.77
A:Q=200:1 3.75 190.93 99.55 191.80
A:Q=90:1 3.62 197.79 99.01 199.78
A:Q=50:1 3.51 203.99 98.23 207.67
A:Q=25:1 3.46 206.94 96.52 214.40
A:Q=12:1 3.85 185.97 93.04 199.89
A:Q=4:1 4.96 144.35 81.90 176.26
A:Q=1:1 7.49 95.59 54.75 174.59
A:Q=1:4 15.69 45.63 27.60 165.32
A:Q=1:15 28.95 24.73 15.16 163.13
A:Q=1:30 35.77 20.02 12.42 161.11
A:Q=1:60 46.15 15.51 10.99 141.19
A:Q=1:100 56.25 12.73 10.40 122.38
6-9 is visible for toxicity test result table, methylsulfonyl bacterium azoles respectively with paclobutrazol, heteroauxin, first piperazine, adjust naphthenic acid in (100000 ~ 1): (1: ~ 100) in scope, the composite co-toxicity coefficient preventing and treating soft rot of cabbage is all greater than 120, shows obvious synergistic function.Especially in (10000 ~ 1): time composite in (1 ~ 30) scope, the CTC of each process is all greater than 160, and synergy is particularly remarkable.
Toxicity Determination embodiment three: (cucumber bacterial angular leaf spot)
Below that methylsulfonyl bacterium azoles is tested with diethyl aminoethyl hexanoate, the basic element of cell division, Nafusaku, hydrocarbon enadenine, the composite Toxicity Determination to cucumber bacterial angular leaf spot of inabenfide respectively.
Be that 108cfumL-1 pathogen adds 0.5mL in each diameter 9cm sterilizing culture dish by bacteria suspension concentration, then pour 15mL into and be cooled in 45 DEG C of gravy peptone medium, fully mix, solidify.At the equidistant Angle Position of 3 Ge Ju center 2.5cm of culture dish bottom marker equilateral triangle, prevent Oxford cup (high 10mm, internal diameter 6mm), drip the medicament dilution of equivalent variable concentrations, 7d is cultivated under 28 DEG C of constant temperature aseptic conditions, measure antibacterial circle diameter, and calculate mean value, the inhibiting rate of antibacterial circle diameter.Carry out statistical analysis with DPS data processing software, calculate the EC of each medicament 50, then press the abundant method of Sun Yun and calculate co-toxicity coefficient (CTC).The results are shown in Table 10 ~ table 14.
The Toxicity Determination result of table 10 methylsulfonyl bacterium azoles and the composite control cucumber bacterial angular leaf spot of diethyl aminoethyl hexanoate
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 7.46 100.00 / /
Diethyl aminoethyl hexanoate (hereinafter referred to as D) 76.37 9.77 / /
A:D=100000:1 6.21 120.13 100.00 120.13
A:D=50000:1 5.70 130.88 100.00 130.88
A:D=25000:1 5.13 145.42 100.00 145.42
A:D=10000:1 4.53 164.68 99.99 164.69
A:D=5000:1 4.38 170.32 99.98 170.35
A:D=2500:1 4.24 175.94 99.96 176.01
A:D=1000:1 4.18 178.47 99.91 178.63
A:D=550:1 3.81 195.80 99.84 196.12
A:D=200:1 3.72 200.54 99.55 201.44
A:D=90:1 3.50 213.14 99.01 215.28
A:D=50:1 3.66 203.83 98.23 207.50
A:D=25:1 3.95 188.86 96.53 195.65
A:D=12:1 4.33 172.29 93.06 185.14
A:D=3.5:1 5.17 144.29 79.95 180.48
A:D=1:1 7.78 95.89 54.88 174.71
A:D=1:4 15.94 46.80 27.81 168.26
A:D=1:15 29.88 24.97 15.41 162.04
A:D=1:30 36.48 20.45 12.68 161.29
A:D=1:60 46.22 16.14 11.25 143.50
A:D=1:100 56.34 13.24 10.66 124.19
Table 11 methylsulfonyl bacterium azoles and the composite Toxicity Determination result of preventing and treating cucumber bacterial stripe of the basic element of cell division
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 7.13 100.00 / /
The basic element of cell division (hereinafter referred to as E) 75.89 9.40 / /
A:E=100000:1 5.80 122.93 100.00 122.93
A:E=50000:1 5.38 132.53 100.00 132.53
A:E=25000:1 5.12 139.26 100.00 139.26
A:E=10000:1 4.23 168.56 99.99 168.57
A:E=5000:1 4.14 172.22 99.98 172.25
A:E=2500:1 3.76 189.63 99.96 189.70
A:E=1000:1 3.65 195.34 99.91 195.52
A:E=550:1 3.54 201.41 99.84 201.74
A:E=200:1 3.41 209.09 99.55 210.04
A:E=90:1 3.35 212.84 99.00 214.98
A:E=50:1 3.69 193.22 98.22 196.72
A:E=25:1 3.71 192.18 96.52 199.12
A:E=12:1 4.28 166.59 93.03 179.07
A:E=3.5:1 5.19 137.38 79.87 172.01
A:E=1:1 7.58 94.06 54.70 171.97
A:E=1:4 15.65 45.56 27.52 165.57
A:E=1:15 28.63 24.90 15.06 165.39
A:E=1:30 36.12 19.74 12.32 160.25
A:E=1:60 45.74 15.59 10.88 143.27
A:E=1:100 57.09 12.49 10.29 121.34
Table 12 methylsulfonyl bacterium azoles and the composite Toxicity Determination result of preventing and treating cucumber bacterial stripe of Nafusaku
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 6.84 100.00 / /
Nafusaku (hereinafter referred to as H) 71.26 9.60 / /
A:H=100000:1 5.66 120.85 100.00 120.85
A:H=50000:1 5.30 129.06 100.00 129.06
A:H=25000:1 4.74 144.30 100.00 144.31
A:H=10000:1 4.18 163.64 99.99 163.65
A:H=5000:1 3.91 174.94 99.98 174.97
A:H=2500:1 3.84 178.13 99.96 178.19
A:H=1000:1 3.76 181.91 99.91 182.08
A:H=550:1 3.63 188.43 99.84 188.74
A:H=200:1 3.56 192.13 99.55 193.00
A:H=90:1 3.45 198.26 99.01 200.25
A:H=50:1 3.14 217.83 98.23 221.77
A:H=25:1 3.23 211.76 96.52 219.39
A:H=12:1 3.91 174.94 93.05 188.01
A:H=3.5:1 4.81 142.20 79.91 177.95
A:H=1:1 7.17 95.40 54.80 174.09
A:H=1:4 14.56 46.98 27.68 169.72
A:H=1:15 27.38 24.98 15.25 163.83
A:H=1:30 33.92 20.17 12.51 161.13
A:H=1:60 45.67 14.98 11.08 135.16
A:H=1:100 54.25 12.61 10.49 120.15
Table 13 methylsulfonyl bacterium azoles and the composite Toxicity Determination result of preventing and treating cucumber bacterial stripe of oxyenadenine
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 6.97 100.00 / /
Oxyenadenine (hereinafter referred to as R) 73.35 9.50 / /
A:R=100000:1 5.72 121.85 100.00 121.85
A:R=50000:1 5.31 131.26 100.00 131.26
A:R=25000:1 4.83 144.31 100.00 144.31
A:R=10000:1 4.28 162.85 99.99 162.87
A:R=5000:1 3.97 175.57 99.98 175.60
A:R=2500:1 3.91 178.26 99.96 178.33
A:R=1000:1 3.84 181.51 99.91 181.67
A:R=550:1 3.79 183.91 99.84 184.21
A:R=200:1 3.69 188.89 99.55 189.74
A:R=90:1 3.61 193.07 99.01 195.01
A:R=50:1 3.24 215.12 98.23 219.01
A:R=25:1 3.35 208.06 96.52 215.56
A:R=12:1 3.96 176.01 93.04 189.18
A:R=3.5:1 4.86 143.42 79.89 179.52
A:R=1:1 7.29 95.61 54.75 174.63
A:R=1:4 14.59 47.77 27.60 173.08
A:R=1:15 27.50 25.35 15.16 167.20
A:R=1:30 34.04 20.48 12.42 164.84
A:R=1:60 45.80 15.22 10.99 138.53
A:R=1:100 54.26 12.85 10.40 123.53
Table 14 methylsulfonyl bacterium azoles and the composite Toxicity Determination result to cucumber bacterial stripe of inabenfide
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 8.01 100.00 / /
Inabenfide (hereinafter referred to as T) 89.19 8.98 / /
A:T=100000:1 6.65 120.45 100.00 120.45
A:T=50000:1 6.14 130.46 100.00 130.46
A:T=25000:1 5.16 155.23 100.00 155.24
A:T=10000:1 4.87 164.48 99.99 164.49
A:T=5000:1 4.70 170.43 99.98 170.46
A:T=2500:1 4.59 174.51 99.96 174.57
A:T=1000:1 4.18 191.63 99.91 191.80
A:T=550:1 4.10 195.37 99.83 195.69
A:T=200:1 3.94 203.30 99.55 204.22
A:T=90:1 3.78 211.90 99.00 214.05
A:T=50:1 3.89 205.91 98.22 209.65
A:T=25:1 4.31 185.85 96.50 192.59
A:T=12:1 4.54 176.43 93.00 189.71
A:T=3.5:1 5.37 149.16 79.77 186.98
A:T=1:1 7.97 100.50 54.49 184.44
A:T=1:4 16.88 47.45 27.18 174.56
A:T=1:15 32.96 24.30 14.67 165.66
A:T=1:30 41.36 19.37 11.92 162.51
A:T=1:60 50.37 15.90 10.47 151.84
A:T=1:100 65.08 12.31 9.88 124.55
10-14 is visible for toxicity test result table, methylsulfonyl bacterium azoles respectively with diethyl aminoethyl hexanoate, the basic element of cell division, Nafusaku, hydrocarbon enadenine, inabenfide in (100000 ~ 1): (1: ~ 100) in scope, the composite co-toxicity coefficient preventing and treating cucumber bacterial stripe is all greater than 120, shows obvious synergistic function.Especially in (10000 ~ 1): time composite in (1 ~ 30) scope, the CTC of each process is all greater than 160, and synergy is particularly remarkable.
Toxicity Determination embodiment four: (bacterial wilt of tomato)
Below that methylsulfonyl bacterium azoles is tested with compound sodium nitrophenolate, heteroauxin, CPPU, Choline Chloride, the composite Toxicity Determination to bacterial wilt of tomato of N-6-benayl aminopurine respectively.
After being activated on NA medium by tobacco bacterial wilt pathogen, be made into bacterium stoste with sterile water, the clump count grown after bacterium stoste is diluted to coated plate 100ul is the bacteria suspension of about 100, for subsequent use.
Get 400ul bacteria suspension and equivalent agricultural chemicals single dose mixes, 100ul is got with liquid-transfering gun, be placed on ready-made NA flat board, with sterilized " L " shape glass bar by even for bacteria suspension coating, cultivate 48h for 28 DEG C, counting clump count, and press formulae discovery bacteriostasis rate, bacterium colony inhibiting rate (%)=(contrast clump count-process clump count)/contrast clump count × 100, often process repetition 4 times, replace pesticide-treated for contrast with sterile water, the result of gained adopts Excel software analysis, calculates the EC of each medicament 50, and calculate co-toxicity coefficient according to the abundant method of Sun Yun.The results are shown in Table 15 ~ table 19.
The Toxicity Determination result of table 15 methylsulfonyl bacterium azoles and the composite control of plant bacterial wilt of compound sodium nitrophenolate
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 12.27 100.00 / /
Compound sodium nitrophenolate (hereinafter referred to as C) 73.88 16.61 / /
A:C=100000:1 9.82 124.95 100.00 124.95
A:C=60000:1 9.03 135.88 100.00 135.88
A:C=30000:1 8.60 142.67 100.00 142.68
A:C=10000:1 7.57 162.09 99.99 162.10
A:C=5000:1 7.49 163.82 99.98 163.85
A:C=2500:1 7.38 166.26 99.97 166.32
A:C=1000:1 7.28 168.54 99.92 168.68
A:C=600:1 7.15 171.61 99.86 171.85
A:C=200:1 6.83 179.65 99.59 180.40
A:C=90:1 6.17 198.87 99.08 200.70
A:C=50:1 6.38 192.32 98.36 195.52
A:C=25:1 6.59 186.19 96.79 192.36
A:C=12:1 7.26 169.01 93.59 180.59
A:C=3.5:1 8.50 144.35 81.47 177.19
A:C=1:1 12.53 97.92 58.30 167.96
A:C=1:4 22.54 54.44 33.29 163.54
A:C=1:15 34.78 35.28 21.82 161.68
A:C=1:30 39.57 31.01 19.30 160.68
A:C=1:60 45.06 27.23 17.98 151.49
A:C=1:100 58.40 21.01 17.43 120.52
The Toxicity Determination result of table 16 methylsulfonyl bacterium azoles and the composite control of plant bacterial wilt of heteroauxin
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 13.65 100.00 / /
Indolebutyric acid (hereinafter referred to as F) 68.39 19.96 / /
A:F=100000:1 11.12 122.75 100.00 122.75
A:F=60000:1 10.27 132.91 100.00 132.91
A:F=30000:1 9.64 141.60 100.00 141.60
A:F=10000:1 8.51 160.40 99.99 160.41
A:F=5000:1 8.43 161.92 99.98 161.95
A:F=2500:1 8.32 164.06 99.97 164.12
A:F=1000:1 8.28 164.86 99.92 164.99
A:F=600:1 8.10 168.52 99.87 168.74
A:F=200:1 8.00 170.63 99.60 171.31
A:F=90:1 7.43 183.71 99.12 185.34
A:F=50:1 7.17 190.38 98.43 193.41
A:F=25:1 7.43 183.71 96.92 189.55
A:F=12:1 7.71 177.04 93.84 188.66
A:F=3.5:1 8.97 152.17 82.21 185.10
A:F=1:1 12.73 107.23 59.98 178.77
A:F=1:4 22.45 60.80 35.97 169.05
A:F=1:15 32.86 41.54 24.96 166.41
A:F=1:30 37.72 36.19 22.54 160.54
A:F=1:60 46.20 29.55 21.27 138.90
A:F=1:100 54.23 25.17 20.75 121.29
The Toxicity Determination result of table 17 methylsulfonyl bacterium azoles and the composite control of plant bacterial wilt of CPPU
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 13.65 100.00 / /
CPPU (hereinafter referred to as K) 68.39 19.96 / /
A:K=100000:1 11.12 122.75 100.00 122.75
A:K=60000:1 10.27 132.91 100.00 132.91
A:K=30000:1 9.64 141.60 100.00 141.60
A:K=10000:1 8.51 160.40 99.99 160.41
A:K=5000:1 8.43 161.92 99.98 161.95
A:K=2500:1 8.32 164.06 99.97 164.12
A:K=1000:1 8.28 164.86 99.92 164.99
A:K=600:1 8.10 168.52 99.87 168.74
A:K=200:1 8.00 170.63 99.60 171.31
A:K=90:1 7.43 183.71 99.12 185.34
A:K=50:1 7.17 190.38 98.43 193.41
A:K=25:1 7.43 183.71 96.92 189.55
A:K=12:1 7.71 177.04 93.84 188.66
A:K=3.5:1 8.97 152.17 82.21 185.10
A:K=1:1 12.73 107.23 59.98 178.77
A:K=1:4 22.45 60.80 35.97 169.05
A:K=1:15 32.86 41.54 24.96 166.41
A:K=1:30 37.72 36.19 22.54 160.54
A:K=1:60 46.20 29.55 21.27 138.90
A:K=1:100 54.23 25.17 20.75 121.29
The Toxicity Determination result of table 18 methylsulfonyl bacterium azoles and the composite control of plant bacterial wilt of Choline Chloride
Composition EC 50(μg/ml) ATI TTI CTC
Methylsulfonyl bacterium azoles (hereinafter referred to as A) 12.69 100.00 / /
Choline Chloride (hereinafter referred to as S) 75.36 16.84 / /
A:S=100000:1 10.54 120.40 100.00 120.40
A:S=60000:1 9.72 130.56 100.00 130.56
A:S=30000:1 8.66 146.54 100.00 146.54
A:S=10000:1 7.78 163.11 99.99 163.12
A:S=5000:1 7.47 169.88 99.98 169.91
A:S=2500:1 7.41 171.26 99.97 171.31
A:S=1000:1 7.37 172.18 99.92 172.33
A:S=600:1 7.17 176.99 99.86 177.23
A:S=200:1 7.09 178.98 99.59 179.73
A:S=90:1 6.92 183.38 99.09 185.07
A:S=50:1 6.74 188.28 98.37 191.40
A:S=25:1 6.49 195.53 96.80 201.99
A:S=12:1 6.86 184.99 93.60 197.63
A:S=3.5:1 8.05 157.64 81.52 193.38
A:S=1:1 12.52 101.36 58.42 173.50
A:S=1:4 21.78 58.26 33.47 174.07
A:S=1:15 35.29 35.96 22.04 163.18
A:S=1:30 40.27 31.51 19.52 161.42
A:S=1:60 45.85 27.68 18.20 152.05
A:S=1:100 58.24 21.79 17.66 123.36
The Toxicity Determination result of table 19 methylsulfonyl bacterium azoles and the composite control of plant bacterial wilt of N-6-benayl aminopurine
15-19 is visible for toxicity test result table, methylsulfonyl bacterium azoles with respectively with compound sodium nitrophenolate, heteroauxin, CPPU, Choline Chloride, N-6-benayl aminopurine in (100000 ~ 1): composite in (1 ~ 100) scope, the CTC value of control of plant bacterial wilt is all greater than 120, shows obvious synergistic effect.Especially in (10000 ~ 1): (1 ~ 30) scope is composite, the CTC of each process is all greater than 160, synergy highly significant.
Land for growing field crops test examples
In order to the control efficiency of clear and definite methylsulfonyl bacterium azoles and the composite control bacterial leaf streak of rice of plant growth regulator, bacterial wilt of tomato, and can the result of clear and definite Toxicity Determination (i.e. synergistic effect) be confirmed in field, present invention applicant at home different regions has carried out a large amount of field trials.Illustrate with several embodiment below.Following methylsulfonyl bacterium azoles is referred to as first sulphur.
Contrast medicament:
Contrast medicament 11:20% methylsulfonyl bacterium azole suspending agent, self-control
Methylsulfonyl bacterium azoles 20%, triphen ethyl phenol APEO 9.0%, xanthans 0.1%, ethylene glycol 3.0%, silicone defoaming agent 0.1%, deionized water are mended to 100%, put into high shear homogeneous emulsifying machine high speed and shear 30 minutes, transport in sand mill, namely circulation sand milling obtains 20% methylsulfonyl bacterium azole suspending agent for 1-3 time again.
Field efficacy embodiment one: the field control effectiveness test of control bacterial leaf streak of rice
Test method and computational methods are with reference to " GR/T 17980.105-2004 pesticide field efficacy medicine test criterion (two) the 105th part: bactericidal agent for preventing and treating bacterial leaf streak of rice ", every plot area 20m2, often process and repeat for 4 times, if clear water is treated to blank, spray pesticide is carried out, interval 7 days second time dispenser in their early stage.Respectively at 7 days, 14 days investigation results after second time medicine before first time medicine, after second time medicine, in units of blade, classification investigation incidence, calculates disease index, preventive effect.The results are shown in Table 20:
Table 20 methylsulfonyl bacterium azoles is the field control effectiveness test result of composite control bacterial leaf streak of rice with brassin lactones, compound sodium nitrophenolate etc. respectively
From test of pesticide effectiveness result table 20, methylsulfonyl bacterium azoles is composite when dosage is no more than single dose dosage with brassin lactones, compound sodium nitrophenolate, diethyl aminoethyl hexanoate respectively, the preventive effect of control bacterial leaf streak of rice is higher than single dose, after second time medicine, the preventive effect of 7 days built agents has at least exceeded 21.38% than single dose, and 14 days after second time medicine can also keep good preventive effect, preventive effect is more than 76.16%, and the lasting period is long.
Field efficacy embodiment two: the field control effectiveness test of control of plant bacterial wilt
Test method: with reference to " pesticide field efficacy medicine test criterion (NY/T1464.32-2010) " regulation application method, first time sprays dispenser when beginning to see diseased plant, and after 10d, second time sprays dispenser.Dispenser twice altogether, each process plot area is 45m2, number of repetition 4 times.After second time dispenser, 10d, 20d investigate whole plant of each community, record total strain number and diseased plant number, calculate diseased plant rate and preventive effect.The results are shown in Table 21:
Table 21 methylsulfonyl bacterium azoles is the field control effectiveness test result of composite water prevention bacterial wilt of tomato with triacontanol, gibberellin etc. respectively
From test of pesticide effectiveness result table 21, methylsulfonyl bacterium azoles is composite when dosage is no more than single dose dosage with triacontanol, gibberellin, CPPU, paclobutrazol, heteroauxin, TrinexAN_SNacethyl, chlormequat respectively, the preventive effect of control of plant bacterial wilt is higher than single dose, after second time medicine, the preventive effect of 10 days built agents has at least exceeded 22.35% than single dose, and synergy is obvious; Within 14 days after second time medicine, can also keep good preventive effect, preventive effect is more than 78.75%, and the lasting period is long.

Claims (9)

1. one kind contains the complex composition of methylsulfonyl bacterium azoles and plant growth regulator, it is characterized in that, described complex composition is made up of methylsulfonyl bacterium azoles and plant growth regulator, the chemical name of described methylsulfonyl bacterium azoles is 2-(to fluorophenyl)-5-mesyl-1, 3, 4-oxadiazole, described plant growth regulator is brassin lactones, compound sodium nitrophenolate, diethyl aminoethyl hexanoate, the basic element of cell division, indolebutyric acid, Nafusaku, triacontanol, gibberellin, CPPU, paclobutrazol, heteroauxin, TrinexAN_SNacethyl, chlormequat, first piperazine, adjust naphthenic acid, oxyenadenine, Choline Chloride, inabenfide, any one in 6-benzyl aminopurine.
2. the complex composition containing methylsulfonyl bacterium azoles and plant growth regulator according to claim 1, it is characterized in that, described methylsulfonyl bacterium azoles and the weight ratio of plant growth regulator are 100:0.001 to 1:100.
3. the complex composition containing methylsulfonyl bacterium azoles and plant growth regulator according to claim 1 and 2, it is characterized in that, described methylsulfonyl bacterium azoles and the weight ratio of plant growth regulator are 100:0.01 to 1:30.
4. contain a preparation for methylsulfonyl bacterium azoles and plant growth regulator, it is characterized in that, described preparation comprises acceptable auxiliary material on the arbitrary described complex composition of claim 1-3 and agricultural chemicals, is then prepared into disinfectant use in agriculture.
5. the preparation containing methylsulfonyl bacterium azoles and plant growth regulator according to claim 4, it is characterized in that, by weight, the weight percentage that described complex composition accounts for described bactericide is 0.1%-80%.
6. the preparation containing methylsulfonyl bacterium azoles and plant growth regulator according to claim 4, it is characterized in that, by weight, the weight percentage that described complex composition accounts for described bactericide is 1%-65%.
7. the preparation containing methylsulfonyl bacterium azoles and plant growth regulator according to claim 4, is characterized in that, on described agricultural chemicals, acceptable auxiliary material is the mixture of a kind of and auxiliary agent in solvent and filler.
8., according to the arbitrary described preparation containing methylsulfonyl bacterium azoles and plant growth regulator of claim 4-7, it is characterized in that, the formulation of described bactericide is wetting powder, water dispersible granules, microemulsion, aqueous emulsion, missible oil, suspending agent or granule.
9. the purposes of the arbitrary described complex composition of claim 1-3 in control crop bacterial disease.
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CN113473854A (en) * 2019-02-26 2021-10-01 先正达农作物保护股份公司 Formulations
CN115843815A (en) * 2022-12-07 2023-03-28 四川易宏欣农业科技有限公司 Plant growth regulator and preparation method thereof
CN115868488A (en) * 2022-10-21 2023-03-31 郑州郑氏化工产品有限公司 Preparation method of microcapsule suspending agent containing fatty acid diethylamino ethanol ester

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CN102204543A (en) * 2011-04-18 2011-10-05 河北省农林科学院粮油作物研究所 Brassinolide and paclobutrazol compound soybean growth regulator
CN102499247A (en) * 2011-10-17 2012-06-20 贵州大学 Oxadiazole sulfone compound for controlling bacterial crop diseases

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CN102204543A (en) * 2011-04-18 2011-10-05 河北省农林科学院粮油作物研究所 Brassinolide and paclobutrazol compound soybean growth regulator
CN102499247A (en) * 2011-10-17 2012-06-20 贵州大学 Oxadiazole sulfone compound for controlling bacterial crop diseases

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CN113473854A (en) * 2019-02-26 2021-10-01 先正达农作物保护股份公司 Formulations
CN113473854B (en) * 2019-02-26 2023-04-04 先正达农作物保护股份公司 Formulations
CN115868488A (en) * 2022-10-21 2023-03-31 郑州郑氏化工产品有限公司 Preparation method of microcapsule suspending agent containing fatty acid diethylamino ethanol ester
CN115868488B (en) * 2022-10-21 2024-03-12 郑州郑氏化工产品有限公司 Preparation method of microcapsule suspending agent containing fatty acid diethylaminoethanol ester
CN115843815A (en) * 2022-12-07 2023-03-28 四川易宏欣农业科技有限公司 Plant growth regulator and preparation method thereof
CN115843815B (en) * 2022-12-07 2023-12-22 孟州农达生化制品有限公司 Plant growth regulator and preparation method thereof

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